EP0013798A1 - Verfahren zum Warmumformen von Aluminium-Magnesium-Legierungen und Aluminium-Magnesium-Legierung - Google Patents

Verfahren zum Warmumformen von Aluminium-Magnesium-Legierungen und Aluminium-Magnesium-Legierung Download PDF

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Publication number
EP0013798A1
EP0013798A1 EP79302232A EP79302232A EP0013798A1 EP 0013798 A1 EP0013798 A1 EP 0013798A1 EP 79302232 A EP79302232 A EP 79302232A EP 79302232 A EP79302232 A EP 79302232A EP 0013798 A1 EP0013798 A1 EP 0013798A1
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Prior art keywords
temperature
alloy
strength
extrusion
aluminium
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EP79302232A
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English (en)
French (fr)
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EP0013798B1 (de
Inventor
Joseph Robert Pickens
Stephen James Donachie
Robert Douglas Schelleng
Thomas John Nichol
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MPD Technology Ltd
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MPD Technology Ltd
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Priority claimed from US05/951,590 external-priority patent/US4297136A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0036Matrix based on Al, Mg, Be or alloys thereof

Definitions

  • the present invention relates to a method for controlling and/or optimizing the strength and workability of dispersion-strengthened aluminium-magnesium alloys.
  • UK Patent 1390857 discloses and claims a process for preparing a mechanically alloyed oxide dispersion-strengthened aluminium or aluminium based alloy powder, and its subsequent consolidation into a formed product.
  • the material produced by this mechanical alloying process has some advantages over conventional dispersion-strengthened aluminium, commonly known as SAP (sintered aluminium product) including greater strength and/or workability. Since the material does not need to be strengthed by age hardening additives which can give susceptibility to stress corrosion cracking, it has potential for certain high corrosion resistance applications, including aircraft skins without cladding, aircraft interior structural members, rifle parts and lightweight automotive parts.
  • UK patent 1390857 also discloses examples of consolidated products of dispersion-strengthened aluminium extruded under conditions varying from extrusion temperatures of between 454 and 482°C at extrusion ratios of 45:1 and 28:1.
  • the ultimate tensile strength (UTS) at room temperature of these products is shown to vary from 312 to 454 MN/m 2 .
  • UTS ultimate tensile strength
  • J H Swartzwelder (INT. J POWDER MET. 3 (3) 1967) reports the behavior of extruded 14 wt. % oxide dispersoid SAP aluminium rod at extrusion ratios varying from 2:1 to 64:1 and 8 wt. % oxide dispersoid SAP aluminium rod at ratios of 2:1 to 76:1.
  • the SAP materials showed a rapid increase in tensile strength as extrusion ratios increased up to about 8;1.
  • the more extensive data obtained for the 8 wt, % dispersoid alloy show a leveling out or slight increase in tensile strength after the initial rapid increase.
  • the present invention is based on the discovery that certain oxide dispersion-strengthened aluminium magnesium alloys can be prepared by mechanical alloying which alloys exhibit improved high strength and corrosion resistance. Furthermore that these alloys have an unconventional response to thermomechanical processing which makes it possible to process the material so that the properties of workability or strength can be optimised, depending on the requirements of the end product.
  • the present invention provides an oxide dispersion-strengthened mechanically-alloyed aluminium based alloy containing from 2 to 8% magnesium, 0.2 to 4% oxygen, up to 21 ⁇ 2% carbon, the balance,apart from impurities and incidental elements,aluminium, and characterised by a tensile strength (UTS)at room temperature of greater than 457 MN/m 2 .
  • UTS tensile strength
  • the alloy will contain from 2 to 5% magnesium, and more preferably 4 to 5%.
  • the alloy contains at least 0.2% carbon.
  • Figure 1 is a graph showing a working temperature strength profile of an oxide dispersion-strengthened mechanically alloyed aluminium-magnesium alloy of the present invention.
  • Figure 2 is a graph showing the effect of extrusion ratio at an extrusion temperature of 343 0 C on room temperature tensile strength (UTS) of an alloy of the present invention (Curve A) and a comparison with the effect on a prior art aluminium alloy, viz. SAP (Curves B and C) containing substantially higher dispersoid levels than the alloy of Curve A.
  • UTS room temperature tensile strength
  • Figure 3 is a graph showing the direct relationship between Brinell hardness (BHN) of compacted billets and room temperature tensile strength (UTS) of rods extruded from each given billet of a dispersion-strengthened mechanically alloyed aluminium of the present invention.
  • the alloys have different dispersoid levels, varying from 1.5 to 4.5 vol. %, and varying strength, but are all extruded at an extrusion ratio of 33.6:1 at two temperature levels, at the lower temperature (Curve D) and a higher temperature level (Curve E).
  • thermomechanical processing conditions to be controlled so that a desired strength of the material realtive to the workability required for a given application can be achieved predictably.
  • an alloy of the present invention which exhibits the desired room temperature tensile strength prior to elevated temperature working.
  • the alloy will be increasingly workable at increasing working temperatures up to incipient melting.
  • the working temperature/strength profile of the selected alloy is then determined. This will exhibit an overall decrease in strength relative to the working temperature which includes a critical transition zone characterised.by a sharp lowering of room temperature strength relative to increased working temperature, as illustrated in Figure 1.
  • the selected alloy is then worked at elevated temperature selected with referance to this transition zone in order to optimize the workability of the alloy and the strength of the worked product.
  • the working temperature-strength profile shows a pattern of behaviour which includes a strength-temperature plateau, shown as 'p' in Figure '1 in which region an increase in working temperature has substantially no affect on strength.
  • the maximum temperature of the plateau is between 371°C and 399°C.
  • TZ critical working temperature-strength transition zone
  • Figure 2 which shows the difference in the effect of extrusion ratio on strength of a material of the present invention (Curve A) from the effect on two samples of prior art aluminium alloys having different oxide dispersoid levels, illustrates that unexpectedly, the initial compacted strength of the present alloys i.e., before thermomechanical treatment, must be greater than the strength required for a particular product. In other words, for alloys of the present invention, the strength of the product will not increase with thermomechanical working in the range studied, as would be expected under certain conditions from the reported behaviour of other dispersion-strengthed aluminium alloys.
  • the temperature strength profiles shown in Figures 1 and 2 may in general be used for oxide dispersion-strengthened mechanically alloyed alloys containing 2 to 5% magnesium, up to 21 ⁇ 2% carbon and 0.2 to 4% oxygen, balance aluminium apart from impurities and incidental elements.
  • the figures show results obtained on a specific composition of alloy in a particular equipment and processed to give a certain initial strength, and to develop a high strength product, hot working should be carried out in the range 343°C to below 400°C, since the critical transition temperature zone is in the range 399°C to 454°C.
  • the processing may be carried out at a higher temperature than the maximum plateau temperatures, but there will be a sacrifice in strength.
  • the ultimate tensile strength of an extruded dispersion-strengthened mechanically alloyed alloy containing from 2 to 7% Mg, up to 21 ⁇ 2% carbon, 0.2 to 4% oxygen, a small but effective amount of dispersoid and the balance, apart from impurities and incidental elements being aluminium can be optimised by employing processing conditions governed by the following relationship:
  • dispersion-strengthened mechanically alloyed aluminium-magnesium with excellent corrosion resistance can be processed to products having an ultimate room temperature tensile strength of greater than 457.1 MN/m 2 (66.3 ksi) and up to 758.3 MN/m 2 (110 ksi) and even higher. Alloys can be prepared having tensile strength in the range of 475.7 to 606.7 MN/m (69 to 88 ksi) with % elongation of 6 to 8.
  • the alloys of the present invention at least a part of the oxygen and carbon are present as dispersoid material.
  • Preferred alloys contain 0.3 to 2% oxygen and . 0.1 to 2.5%. or more preferably 0.2 to 2% carbon.
  • the alloys may contain incidental elements in addition to those specified for the purpose of solid solution hardening or age hardening the alloy and to provide other specific properties as long as they do not interfere with the desired properties of the alloy for its ultimate purpose.
  • the magnesium content of the alloys provides strength, corrosion resistance, good fatigue resistance and low density.
  • Incidental elements which may be added for additional strength are Li, Cr, Si, Zn, Ni, Ti, Zr, Co, Cu and Mn. The use of these additives to aluminium alloys is well known in the art.
  • the dispersoid is an oxide, but it may also contain carbon, silicon, a carbide, a silicide, aluminide, an insoluble metal or an intermetallic which is stable in the aluminium matrix at the ultimate temperature of service.
  • examples of dispersoids are alumina, magnesia, thoria, yttria, rare earth metal oxides, aluminium carbide,graphite, iron alum i n i de .
  • the dispersoid for example Al 2 O 3 , MgO and/or C may be added to the composition in dispersoid form, i.e. as a powder, or may be formed in-situ, preferably during the production of the mechanically alloyed powder.
  • the dispersoids may be present in the range of_a small but effective amount to 81 ⁇ 2 volume %, but preferably the dispersoid level is as low as possible consistent with desired strength.
  • alloys having strength greater than 457 MN/m 2 contain 1 up to but less than 7 v/o dispersoid, and preferably with a minimum of 2 v/o.
  • the oxide dispersoid is present in an amount of less than 5 v/o.
  • Alloys of the present invention are produced in powder form by a mechanical alloying technique, that is a high energy milling process as described in U.K. Patent Nos. 1 265 343 and 1 390 857. Briefly, alloy powder is prepared by subjecting a powder charge to dry, high energy milling in the presence of a grinding media, e.g. balls, and a weld-retarding amount of a surfactive agent or a carbon-contributing agent, e.g.
  • the surfactive agent is preferably an organic material such as organic acids, alcohols, heptanes, aldehydes and ethers.
  • the formation of dispersion-strengthened mechanically alloyed aluminium is given in detail in U.K. Patent No. 1 390 857.
  • the powder is prepared in an attritor using a ball-to-powder ratio of 15:1 to 60:1.
  • the carbon-contributing agents are methanol, stearic acid, and graphite. Carbon from these organic compounds is incorporated in the powder, and it contributes to the total dispersoid content.
  • a compaction step may or may not be used.
  • various gases such as H 2 or H20, may be picked up by the powder particles, and if they are not removed before hot working, the material may blister.
  • Degassing must be carried out at a high temperature, e.g. in the range of 288 to 566°C. Degassing may be accomplished before compacting the powder, e.g. by placing the powder in a metal can and evacuating the can under Vacuum at an elevated temperature, After degassing the can may be sealed and hot compacted against a blank die in an extrusion press. The can material may be subsequently removed by machining, leaving a fully dense billet for further working.
  • the material may be degassed as a loose powder under an inert gas cover at an elevated temperature, or a billet compacted at room temperature to less than theoretical density, e.g 85% theoretical density, may be annealed under argon to remove gases.
  • a time-temperature interrelationship is involved.
  • the time-temperature combination is chosen to minimize loss of strength in the powder and for reasons of cost it is preferred to work materials at the lowest temperature possible consistent with other factors.
  • thermomechanical processing applied to alloys of the present invention is fixed by commercial equipment available and cost considerations.
  • the present invention allows such fixed conditions to be taken into account and allows variables such as composition and treatment of powders and consolidation conditions to be adjusted to optimise workability during processing and strength in the finished product to suit a particular end use.
  • Samples having the nominal compositions of TABLE I were prepared by high energy milling in a 15.1, 113.5 or 378.5 litre attritor for 6 to 16 hours at a ball-to-powder ratio of from 20:1 to 24:1 by weight in a nitrogen or air atmosphere in the presence of either methanol or stearic acid.
  • Compositions given in the examples are in weight % except for dispersoid levels which are given in volume %.
  • This example illustrates the effect degassing temperature has on room temperature strength and ductility of extruded rod.
  • Two cans of powder Sample A were compacted and degassed, one at 510°C and the other at 427 0 C for a time of 3 hours each. Both cans were extruded to 15.9 mm diameter rod at 427 0 C at an extrusion ratio (E/R) of 33.6:1.
  • Two cans of powder Sample B were degassed for 3 hours, one at 566°C and the other at 510°C. After degassing the second two samples were rolled to 20.3 mm diameter plate at 427 o C. Room temperature tensile and ductility tests were performed on the resultant plates. Results are shown in Table II.
  • the data for Powder Type A show that there was an increase in strength with either or both decrease in degas and compaction temperatures.
  • the data for Powder Type B indicate that increased degassing temperature appears to be the controlling factor.
  • This example illustrates the effect of temperature of thermomechanical treatment on strength of dispersion-strengthened mechanically alloyed alloy samples having the nominal composition and the powder processing conditions of powder Type B.
  • Figure 1 shows the unexpected effect of extrusion temperature on the room temperature ultimate tensile strength (UTS) of a dispersion-strengthened mechanically alloyed allay of the invention.
  • the pattern of behaviour includes a strength temperature plateau "P", which illustrates that an increase in working temperature from 288° C to a maximum temperature which is roughly 399°C has substantially no affect on strength.
  • TZ critical working temperature-strength zone
  • This example illustrates the effect of extrusion ratio on strength of dispersion-strengthened mechanically alloyed alloy samples of this invention, and it shows a comparison with prior art materials.
  • Figures 1 and 2 illustrate the unexpected strength- thermomechanical processing interrelationship of alloys of this invention, the understanding of which constitutes a useful means of controlling the properties of dispersion-strengthened mechanically alloyed aluminium-magnesium alloys.
  • Seventy-eight samples of dispersion-strengthened mechanically alloyed aluminium 4-5 wt. % magnesium were prepared essentially comparable to powder samples A, B and C, but containing various amounts of oxygen and carbon.
  • Degassing temperature was 510°C unless otherwise indicated.
  • Compaction temperatures were varied from 288 0 to 566°C, the compacted powders were extruded to 25.4 mm to 9.5 mm rod at extrusion temperatures varying from 288° to 510°C and extrusion ratios from 13.1:1, to 93.4:1.
  • the compositions contained, in addition to aluminium and magnesium, 0.8 to 2 wt. % oxygen, and 0.2 to 1.9 wt. % carbon.
  • the oxide dispersoid varied from 1.7 to 3.4 vol. %.
  • the carbide dispersoid varied from about 0.8 to about 5.8 vol. %.
  • the data is tabulated in TABLE III, which shows actual room temperature tensile strength of samples. It was found that the actual room temperature tensile strength varied from theoretical calculated from the equation given above by approximately 42.7 to 50. 3 MN/m 2 .
  • the following example shows how the knowledge of the effect of degassing time on tensile properties can be used to control properties of the final product.
  • Billet 2 which had a shorter time at the higher degassing temperature has a substantially increased tensile strength, of the finished product by over 124 MN/m 2 .
  • This example illustrates the use of processing information in accordance with the present invention.
  • powder Type D is to be used in a very high strength condition, e.g. for lightweight parts which are to be machined out of the alloy it may be processed as follows:
  • the powder is degassed at 510°C to ensure that all detectable hydrogen is removed and degassing is continued for 4 hours.
  • the additional hour of degassing causes sufficient softening to occur so that extrusions of a 33.6:1 ratio will not be high in strength.
  • the hardness of the compacted billet (176 BHN 500 kg load) indicates that strength will be greater than 620 MN/m 2 if extruded at 343°C at a ratio of.33.6:1.
  • the extrusion is carried out at 343 0 C and properties are as follows:
  • This example illustrates the increased workability with increased working temperature of aluminium-based alloys of the present invention.
  • This sample illustrates the preparation of an alloy of the present invention in the form of sheet.
  • This example illustrates the high corrosion resistance of mechanically alloyed aluminium-magnesium alloys of the present invention.
  • a mechanically alloyed aluminium-magnesium alloy having the composition of Powder Type F degassed at 427°C and compacted at 399°C was rolled to 20.3 mm plate. The sample was exposed to 9.0-days of alternate immersion in a 3.5% NaCl solution.
  • One sample of commercial alloy 7050-T-7651 and one sample of 5083-H-1112 were subjected to the same alternate immersion test.
  • aluminium alloys of the 7000 series have relatively high strength, poor corrosion resistance and the aluminium alloys of the 5000 series have low strength but excellent corrosion resistance.
  • strength and corrosion resistance of the alloy of the present invention with the commercial alloys of the 7000 and 5000 series, it was found that the present alloy had corrosion resistance at least as good as the alloy of the 5000 series and strength approaching that of the 7000 series alloy.
  • This example shows the effect of Mg content on stress corrosion cracking (SCC) resistance of mechanically alloyed aluminium-magnesium alloys of the invention, when exposed to an alternate immersion test.
  • SCC stress corrosion cracking
  • test specimens were in the form of C-rings machined so that stressing was oriented with the short transverse direction.
  • the specimens were exposed for up to 120 days in an alternate immersion test which consisted of a 10-minute immersion in a neutral 3.5% NaCl solution at ambient temperature and a 50-minute drying cycle each hour. Ten litres of solution were used. During the drying period a fan was used to provide a constant flow of air across the samples.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
EP79302232A 1978-10-16 1979-10-16 Verfahren zum Warmumformen von Aluminium-Magnesium-Legierungen und Aluminium-Magnesium-Legierung Expired EP0013798B1 (de)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US951590 1978-10-16
US05/951,590 US4297136A (en) 1978-10-16 1978-10-16 High strength aluminum alloy and process
US81868 1979-10-04
US06/081,868 US4292079A (en) 1978-10-16 1979-10-04 High strength aluminum alloy and process

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EP0013798A1 true EP0013798A1 (de) 1980-08-06
EP0013798B1 EP0013798B1 (de) 1984-02-22

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0194700A2 (de) * 1985-03-15 1986-09-17 Inco Alloys International, Inc. Aluminiumlegierungen
EP0244949A1 (de) * 1986-04-04 1987-11-11 Inco Alloys International, Inc. Herstellung einer stabilen Karbid enthaltenden Aluminiumlegierung durch mechanisches Legieren
US4753690A (en) * 1986-08-13 1988-06-28 Amax Inc. Method for producing composite material having an aluminum alloy matrix with a silicon carbide reinforcement
EP0358822A1 (de) * 1987-03-09 1990-03-21 Exxon Research And Engineering Company Dispersionsgehärtete Pulver und stranggepresste Formkörper aus diesen Pulvern
WO1994012677A1 (de) * 1992-11-20 1994-06-09 'techma' Gesellschaft Mit Beschränkter Haftung Aluminiumlegierung

Families Citing this family (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0035070B1 (de) * 1980-03-03 1985-05-15 BBC Aktiengesellschaft Brown, Boveri & Cie. Gedächtnislegierung auf der Basis eines kupferreichen oder nickelreichen Mischkristalls
US4600556A (en) * 1983-08-08 1986-07-15 Inco Alloys International, Inc. Dispersion strengthened mechanically alloyed Al-Mg-Li
US4613386A (en) * 1984-01-26 1986-09-23 The Dow Chemical Company Method of making corrosion resistant magnesium and aluminum oxyalloys
US4758273A (en) * 1984-10-23 1988-07-19 Inco Alloys International, Inc. Dispersion strengthened aluminum alloys
US4643780A (en) * 1984-10-23 1987-02-17 Inco Alloys International, Inc. Method for producing dispersion strengthened aluminum alloys and product
US4627959A (en) * 1985-06-18 1986-12-09 Inco Alloys International, Inc. Production of mechanically alloyed powder
US4668470A (en) * 1985-12-16 1987-05-26 Inco Alloys International, Inc. Formation of intermetallic and intermetallic-type precursor alloys for subsequent mechanical alloying applications
JPS6365045A (ja) * 1986-09-04 1988-03-23 Showa Alum Corp 粒子分散形Al基複合材
US4847044A (en) * 1988-04-18 1989-07-11 Rockwell International Corporation Method of fabricating a metal aluminide composite
US4832734A (en) * 1988-05-06 1989-05-23 Inco Alloys International, Inc. Hot working aluminum-base alloys
US5240521A (en) * 1991-07-12 1993-08-31 Inco Alloys International, Inc. Heat treatment for dispersion strengthened aluminum-base alloy
US5367048A (en) * 1992-06-19 1994-11-22 University Technologies International Inc. Polymer alloy material and process for production thereof
EP0577436B1 (de) * 1992-07-02 1997-12-03 Sumitomo Electric Industries, Limited Stickstoff-verdichtete Sinterlegierungen auf Aluminium-Basis und Verfahren zur Herstellung
US5511603A (en) * 1993-03-26 1996-04-30 Chesapeake Composites Corporation Machinable metal-matrix composite and liquid metal infiltration process for making same
DE4418600C2 (de) * 1994-05-27 1997-03-20 Fraunhofer Ges Forschung Verfahren zur Herstellung von dispersionsverstärkten metallischen Werkstoffen, insbesondere Kupfer und Silber
US20030056928A1 (en) * 2000-03-13 2003-03-27 Takashi Kubota Method for producing composite material and composite material produced thereby
US7217388B2 (en) * 2001-04-13 2007-05-15 Tanaka Kikinzoku Kogyo K.K. Method for preparing reinforced platinum material
US20060153728A1 (en) * 2005-01-10 2006-07-13 Schoenung Julie M Synthesis of bulk, fully dense nanostructured metals and metal matrix composites
CN101611210B (zh) * 2007-01-08 2013-05-15 霍利贝顿能源服务公司 金属间铝化物多晶金刚石复合片(pdc)切削部件
US8333853B2 (en) * 2009-01-16 2012-12-18 Alcoa Inc. Aging of aluminum alloys for improved combination of fatigue performance and strength
US10058917B2 (en) 2014-12-16 2018-08-28 Gamma Technology, LLC Incorporation of nano-size particles into aluminum or other light metals by decoration of micron size particles

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GB1390857A (en) * 1971-07-06 1975-04-16 Int Nickel Ltd Composite powder and the production thereof

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FR1578586A (de) * 1967-08-31 1969-08-14
GB1390857A (en) * 1971-07-06 1975-04-16 Int Nickel Ltd Composite powder and the production thereof

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THE INTERNATIONAL JOURNAL OF POWDER METALLURGY & POWDER TECHNOLOGY, vol. 10, no. 3, July 1974, Baltimore, USA, P.J.M. CHARE et al.: "Densification and properties of extruded Al-Zn-Mg atomised powder", pages 203-215. *
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0194700A2 (de) * 1985-03-15 1986-09-17 Inco Alloys International, Inc. Aluminiumlegierungen
EP0194700A3 (de) * 1985-03-15 1988-01-07 Inco Alloys International, Inc. Aluminiumlegierungen
EP0244949A1 (de) * 1986-04-04 1987-11-11 Inco Alloys International, Inc. Herstellung einer stabilen Karbid enthaltenden Aluminiumlegierung durch mechanisches Legieren
US4753690A (en) * 1986-08-13 1988-06-28 Amax Inc. Method for producing composite material having an aluminum alloy matrix with a silicon carbide reinforcement
EP0358822A1 (de) * 1987-03-09 1990-03-21 Exxon Research And Engineering Company Dispersionsgehärtete Pulver und stranggepresste Formkörper aus diesen Pulvern
WO1994012677A1 (de) * 1992-11-20 1994-06-09 'techma' Gesellschaft Mit Beschränkter Haftung Aluminiumlegierung

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US4292079A (en) 1981-09-29
EP0013798B1 (de) 1984-02-22
CA1141568A (en) 1983-02-22

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